CN108461712B - Potassium/potassium ferrite/Prussian blue solid-state battery and preparation method thereof - Google Patents
Potassium/potassium ferrite/Prussian blue solid-state battery and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a potassium/potassium ferrite/Prussian blue solid-state battery and a preparation method thereof, belonging to the technical field of electrochemistry. The invention provides a potassium/potassium ferrite/Prussian blue solid-state battery which is prepared by mixing Prussian blue, potassium ferrite, acetylene black, polyvinylidene fluoride and N-methyl-2-pyrrolidone in a mass ratio of 50-60: 10-30: 5-20, fully grinding, coating the obtained mixture on an aluminum foil, and carrying out vacuum drying at 120 ℃ for 24-30 hours to obtain Prussian blue sheets; pressing potassium ferrite into a sheet, and sintering at 650-750 ℃ to obtain the electrolyte sheet. And stacking the Prussian blue sheet, the electrolyte sheet and the metal potassium sheet together to assemble the potassium/potassium ferrite/Prussian blue solid-state battery. The potassium/potassium ferrite/Prussian blue solid-state battery has the advantages of high safety, high charge and discharge rate, low cost and the like.
Description
Technical Field
The invention belongs to the technical field of electrochemistry, and particularly relates to a potassium/Prussian blue battery and a preparation method thereof.
Background
The practical application of the battery in our lives plays important roles including electronic consumption, power supply to automobiles, fixed load for intermittent renewable energy power generation and the like. However, the current commercialized battery can not meet the demand of the rapid development of society, such as portable electronic devices, electric vehicles, network energy storage systems, and the like. The development of batteries now requires higher energy density, longer cycle life, and is safer and cheaper. Most of the research on batteries during the past 20 years has focused on liquid electrolyte systems, which have poor electrochemical and thermal stability, low ion selectivity, and poor safety, even though they have high conductivity and excellent wettability of electrode surfaces. The replacement of liquid electrolytes with solid electrolytes not only overcomes the problem of liquid electrolyte permanence, but also provides the possibility for developing new chemical batteries.
Based on this, the use of solid electrolyte batteries has been rapidly growing. Lithium is the lightest alkali metal, which means that lithium has a high specific gram capacity. Energy is the specific capacity x voltage, so the lithium-related battery technology energy density is almost the highest among the current batteries. In addition, the lithium ion battery has the advantage of small volume. Therefore, the method rapidly promotes the revolutionary development of the fields such as smart phones, cameras, notebook computers and electric vehicles after the industrialization of the 90 s.
The development of lithium batteries seems to meet a bottleneck period at present, the energy density is slowly improved, the cost is not rapidly reduced, and the lithium batteries are challenged in the aspects of quick charging, temperature range adaptation, larger-scale deployment application (electric vehicles and energy storage) and resource abundance. Therefore, people are always searching for a new secondary battery technology to make up for the defects of the lithium battery. Potassium metal has a much larger storage capacity than lithium and is cheaper. If the metal potassium is used as a material for manufacturing the battery, the production cost of the battery can be greatly reduced.
Although the radius of the potassium ion is larger, the potassium ion and lithium belong to alkali metal elements, and the potassium ion has similar chemical properties and has similar oxidation-reduction potential to lithium ions. Potassium ions can be well inserted into and removed from Prussian blue materials, so that potassium is used for replacing lithium, the development of a potassium ion battery is completely feasible, and the potassium battery has more potential in the aspect of large-scale energy storage power grid application by integrating factors such as price, reserves and electrochemical properties. Potassium ferrite (K)2Fe4O7) (Yuanhongming et al, potassium ferrite and its preparation method: chinese CN201510245772.6) is a ferrite material having a three-dimensional channel structure, and the ionic conductivity of the material at room temperature is 10-2S/cm or more, and electron conductivity of less than 10-7S/cm, is a very potential electrolyte material.
Disclosure of Invention
The invention aims to solve the technical problems that the solid electrolyte replaces the liquid electrolyte so that the battery can be charged and discharged rapidly, and the safety is improved; the invention provides a potassium/potassium ferrite/Prussian blue solid-state battery with high charge-discharge rate, high safety and low price and a preparation method thereof.
The invention adopts the technical scheme that a potassium/potassium ferrite/Prussian blue solid-state battery takes a Prussian blue sheet as a positive electrode and a potassium ferrite sheet (K)2Fe4O7) Is electrolyte, and the metal potassium sheet is a negative electrode; the preparation method of the potassium/potassium ferrite/Prussian blue solid-state battery is that a Prussian blue sheet, a potassium ferrite sheet and a metal potassium sheet are stacked together according to the sequence of a positive electrode, an electrolyte and a negative electrode.
The potassium/potassium ferrite/Prussian blue solid-state battery is characterized in that a Prussian blue sheet is used as a positive electrode, potassium ferrite is used as an electrolyte, and a metal potassium sheet is used as a negative electrode.
The molecular formula of the potassium ferrite is K2Fe4O7(ii) a The model of the potassium/potassium ferrite/Prussian blue solid-state battery is preferably 2032 type, 2016 type or 2025 type.
The preparation method of the potassium/potassium ferrite/Prussian blue all-solid-state battery comprises the following steps:
(1) mixing Prussian blue, potassium ferrite 1, acetylene black, polyvinylidene fluoride (PVDF) and N-methyl-2-pyrrolidone (NMP), fully grinding and uniformly mixing in a mortar to obtain a mixture; coating the mixture on an aluminum foil, and carrying out vacuum drying at 120 ℃ for 24-30 hours to obtain Prussian blue tablets; the mass ratio of the Prussian blue to the potassium ferrite 1 to the acetylene black to the PVDF to the N-methyl-2-pyrrolidone is 50-60: 10-30: 5-20; the Prussian blue is preferably KFeFe (CN)6Or KFeMn (CN)6(ii) a The molecular formula of the potassium ferrite 1 is K2Fe4O7；
(2) Pressing potassium ferrite 2 into a sheet, and sintering at 650-750 ℃ to obtain a potassium ferrite sheet; the molecular formula of the potassium ferrite 2 is K2Fe4O7；
(3) And stacking the Prussian blue sheet, the potassium ferrite sheet and the metal potassium sheet together to assemble the potassium/potassium ferrite/Prussian blue solid-state battery.
The potassium/potassium ferrite/Prussian blue solid-state battery has good charge and discharge performance and high charge and discharge rate (the specific capacity reaches 65mAh/g when the potassium/potassium ferrite/Prussian blue solid-state battery is charged and discharged at the rate of 10C), and the potassium/potassium ferrite/Prussian blue solid-state battery is a potential solid-state potassium ion battery (the charge and discharge rate of a common liquid electrolyte battery is below 1C) with high safety and high charge and discharge rate.
Drawings
FIG. 1K2Fe4O7The structure of (1).
FIG. 2K2Fe4O7Voltammetric cycling profile of (a).
FIG. 3 KFeFe (CN) of example 16The charge-discharge curve of the 2032 type potassium/potassium ferrite/prussian blue solid-state battery 1 as the positive electrode at different rates.
FIG. 4 KFeFe (CN) of example 16The 2032 type potassium/potassium ferrite/Prussian blue solid-state battery 1 as the anode is connected with a light-emitting picture of a red light diode.
FIG. 5 embodiment 2 by KFeMn (CN)6The positive electrode potassium/potassium ferrite/prussian blue solid-state battery 2 was a charge-discharge curve at different rates.
Detailed Description
The present invention will be described below with reference to specific embodiments, but the present invention is not limited thereto.
Example 1
(1) 1.2g KFeFe (CN)60.6g of a compound having the molecular formula K2Fe4O7Mixing 1 g of potassium ferrite, 0.2g of acetylene black, 0.2g of polyvinylidene fluoride (PVDF) and 0.5g of N-methyl-2-pyrrolidone (NMP), fully grinding and uniformly mixing in a mortar to obtain a mixture; coating the mixture on an aluminum foil, and performing vacuum drying at 120 ℃ for 24 hours to obtain a Prussian blue tablet 2;
(2) pressing potassium ferrite 2 into slices, and sintering at 650 ℃ to obtain potassium ferrite slices;
(3) a prussian blue sheet, a potassium ferrite sheet, and a potassium metal sheet were stacked together to assemble a 2032 type potassium/potassium ferrite/prussian blue solid-state battery 1.
The potassium ferrite used in the invention is a novel electrolyte material with a three-dimensional network structure, and the structure of the electrolyte material is shown in figure 1.
The electrochemical stability of the potassium ferrite material is determined by cyclic voltammetry, and the material is not decomposed at 0-5V, as shown in figure 2.
FIG. 3 shows KFeFe (CN)6The charge-discharge curve of the 2032 type potassium/potassium ferrite/prussian blue solid-state battery 1 as the positive electrode at different rates. Fig. 3 shows that the first charge and discharge capacity of the 2032 type potassium/potassium ferrite/prussian blue solid-state battery 1 at a rate of 1C is 79mAh/g, the capacity at 10C is 65mAh/g, and the charge and discharge rate is relatively fast.
FIG. 4 shows KFeFe (CN)6The 2032 type potassium/potassium ferrite/Prussian blue solid-state battery 1 as the anode is connected with a light-emitting picture of a red light diode, which shows that the battery can provide stable voltage to enable the red light diode to emit light.
Example 2
(1) 1, g KFeFe (CN)60.2g of formula K2Fe4O7Mixing 1 g of potassium ferrite, 0.4g of acetylene black, 0.4g of polyvinylidene fluoride (PVDF) and 0.5g of N-methyl-2-pyrrolidone (NMP), fully grinding and uniformly mixing in a mortar to obtain a mixture; coating the mixture on an aluminum foil, and performing vacuum drying at 120 ℃ for 24 hours to obtain a Prussian blue tablet 2;
(2) the molecular formula is K2Fe4O7Pressing the potassium ferrite 2 into slices, and sintering at 650 ℃ to obtain potassium ferrite slices 2;
(3) the prussian blue sheet 2, the potassium ferrite sheet 2 and the metal potassium sheet were stacked together to assemble a 2032 type potassium/potassium ferrite/prussian blue solid-state battery 2.
The specific capacity of the 2032 type potassium/potassium ferrite/Prussian blue solid-state battery 2 which is charged and discharged for the first time at the rate of 1C is 70 mAh/g.
Example 3
(1) 1.2g KFeFe (CN)60.6g of a compound having the molecular formula K2Fe4O7Potassium ferrite 1, 0.2g acetylene black, 0.2g polyvinylidene fluoride (PVDF) and 0.5g N-methyl-2-pyrrolidone (NMP) were mixed, sufficiently ground and mixed in a mortarHomogenizing to obtain a mixture; coating the mixture on an aluminum foil, and performing vacuum drying at 120 ℃ for 24 hours to obtain a Prussian blue sheet 3;
(2) the molecular formula is K2Fe4O7Pressing the potassium ferrite 2 into slices, and sintering at 650 ℃ to obtain potassium ferrite slices;
(3) the prussian blue sheet 3, the potassium ferrite sheet 3, and the metal potassium sheet were stacked together to assemble a 2016 type potassium/potassium ferrite/prussian blue solid-state battery 3.
Example 4
(1) 1.2g KFeFe (CN)60.6g of a compound having the molecular formula K2Fe4O7Mixing 1 g of potassium ferrite, 0.2g of acetylene black, 0.2g of polyvinylidene fluoride (PVDF) and 0.5g of N-methyl-2-pyrrolidone (NMP), fully grinding and uniformly mixing in a mortar to obtain a mixture; coating the mixture on an aluminum foil, and performing vacuum drying at 120 ℃ for 24 hours to obtain a Prussian blue sheet 4;
(2) the molecular formula is K2Fe4O7Pressing the potassium ferrite 2 into slices, and sintering at 700 ℃ to obtain potassium ferrite slices 4;
(3) the prussian blue sheet, the potassium ferrite sheet, and the potassium metal sheet were stacked together to assemble a 2025 type potassium/potassium ferrite/prussian blue solid-state battery 4.
Example 5
Sintered at 750 ℃ with the molecular formula K2Fe4O7Example 1 was repeated to obtain a 2032 type potassium/potassium ferrite/prussian blue solid-state battery 5.
Example 6
With 1.2g KFeMn (CN)6Instead of 1.2g KFeFe (CN)6Example 1 was repeated to obtain 2032-type battery 6.
FIG. 5 shows a structure represented by KFeMn (CN)6The charge and discharge curves at different rates for the battery, which is the positive electrode material, show that the battery has a faster charge and discharge rate (51 mAh/g specific capacity at 10C) and decays faster than the battery of example 1.
Example 7
Sintered at 750 ℃ with the molecular formula K2Fe4O7 Potassium ferrite tabletExample 6 was repeated to obtain a 2032 type potassium/potassium ferrite/prussian blue solid-state battery 7.
Example 8
A 2016 type potassium/potassium ferrite/prussian blue solid-state battery 8 was produced by the method of example 1.
Example 9
A 2025 type potassium/potassium ferrite/prussian blue solid-state battery 9 was produced by the method of example 1.
The foregoing is a more detailed description of the invention in connection with specific preferred embodiments and it is not intended that the invention be limited to these specific details. It should be understood by those skilled in the art that various changes and substitutions may be made in accordance with the technical solution and the inventive concept of the present invention, and the same properties or uses should be considered as the protection scope of the present invention.
Claims (1)
1. A preparation method of a potassium/potassium ferrite/Prussian blue all-solid-state battery takes a Prussian blue sheet as a positive electrode, potassium ferrite as an electrolyte and a metal potassium sheet as a negative electrode; the method is characterized in that:
(1) mixing Prussian blue, potassium ferrite 1, acetylene black, polyvinylidene fluoride and N-methyl-2-pyrrolidone, fully grinding and uniformly mixing in a mortar to obtain a mixture; coating the mixture on an aluminum foil, and carrying out vacuum drying at 120 ℃ for 24-30 hours to obtain Prussian blue tablets; the mass ratio of the Prussian blue to the potassium ferrite 1 to the acetylene black to the polyvinylidene fluoride and the N-methyl-2-pyrrolidone is 50-60: 10-30: 5-20; the Prussian blue is KFeFe (CN)6Or KFeMn (CN)6(ii) a The molecular formula of the potassium ferrite 1 is K2Fe4O7；
(2) Pressing potassium ferrite 2 into a sheet, and sintering at 650-750 ℃ to obtain a potassium ferrite sheet; the molecular formula of the potassium ferrite 2 is K2Fe4O7；
(3) Stacking a Prussian blue sheet, a potassium ferrite sheet and a metal potassium sheet together to assemble a potassium/potassium ferrite/Prussian blue solid-state battery; the types of the potassium/potassium ferrite/Prussian blue solid-state batteries are 2032 type, 2016 type or 2025 type.
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| CN110031526B (en) * | 2019-04-23 | 2021-03-19 | 吉林大学 | Based on K2Fe4O7Dopamine enzyme-free sensor of electrode, preparation method and application thereof |
| CN110526697B (en) * | 2019-06-27 | 2021-12-03 | 宁波大学 | Liquid phase synthesis K6.25Be0.1Al0.1P0.05Ti0.05Si1.7O7Potassium fast ion conductor and preparation method thereof |
| CN110526699B (en) * | 2019-06-27 | 2021-12-07 | 宁波大学 | Liquid phase synthesis K2.25MgBe0.1Al0.1P0.05Ti0.05Si4.7O12Potassium fast ion conductor and preparation method thereof |
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